As disclosed in U.S. Pat. No. 4,590,010 (Ramachandran et al.) and copending applications Ser. No. 808,304 (Lin et al.), filed Dec. 12, 1985, and Ser. Nos. 854,084 (Davidson I) and 854,085 (Davidson II), filed Apr. 21, 1986, it is known that (trifluoromethyl)naphthalenes can be prepared by reacting a corresponding halonaphthalene with a trifluoroacetate salt in the presence of cuprous iodide and a dipolar aprotic solvent. The products of these reactions can be recovered by conventional techniques involving filtration and centrifugation, but such recovery processes have proved to be unsatisfactory. What is needed is a recovery process which separates the trifluoromethylated product from the other ingredients of the synthesis mixture without the need for a troublesome filtration step and which accomplishes the separation in such a way as to facilitate recycling of the solvent and cuprous iodide.